Plgel columns

Manufactured by Agilent Technologies

Sourced in United States

PLgel columns are analytical chromatography columns designed for the separation and analysis of polymers. They are used in size exclusion chromatography (SEC) and gel permeation chromatography (GPC) applications to determine the molecular weight distribution and other characteristics of polymeric materials.

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Lab products found in correlation

410 differential refractometer, by Waters Corporation (3 mentions) Dawn eos multi angle laser light scattering detector, by Waters Corporation (3 mentions) L lactide, by Thermo Fisher Scientific (2 mentions) Stainless steel glovebox, by MBraun (2 mentions) Infinity gpcsystem, by Agilent Technologies (2 mentions) Polystyrene standards, by Polymer Laboratories (1 mentions) Ri 2031 plus, by Jasco (1 mentions) As 2055plus autosampler, by Jasco (1 mentions) Lc 2000plus, by Jasco (1 mentions) Alliance 2695 separation module, by Waters Corporation (1 mentions) Avance 300 mhz spectrometer, by Bruker (1 mentions) Ultrahydrogel column, by Waters Corporation (1 mentions) 500 mhz nmr spectrometer, by Agilent Technologies (1 mentions) Rac lactide, by Thermo Fisher Scientific (1 mentions) Vertex 70, by Bruker (1 mentions) Dsc 822, by Mettler Toledo (1 mentions)

9 protocols using plgel columns

Determining Polymer Molecular Weights

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Example 9

MALLS, i.e. Multi-angle Laser Light Scattering, was used in conjunction with GPC to determine the molecular weights and polydispersity of the polymers. The system used a Wyatt DAWN EOS multi-angle laser light scattering detector (k=690 nm) with a Waters 410 differential refractometer (RI) (k=930 nm) connected in series. Chromatographic separation by the size exclusion principle (largest comes out first) was achieved by using four Agilent PLgel columns (pore sizes 10³, 10⁴, 10⁵, and 10⁶Å) connected in series. Degassed THF was used as the mobile phase with a temperature of 35° C. and a flow rate of 0.9 ml/min. The time for complete elution through the system was 50 min, and MALLS and RI data were recorded at 5 Hz.

Samples were prepared by dissolving 5 mg of polymer in 1 ml of THF and filtering the solution through 0.45 μm PTFE membrane syringe filters immediately before injection. An injection volume of 20 μl was used. The data were analyzed by Wyatt Astra Software (version 5.3.4) using the Zimm fitting formula with dn/dc=0.125 for PCOD in THF to obtain weight-average molecular weight (M_w) for each polymer reported.

US10427995B2. Molecular sieves mediated unsaturated hydrocarbon separation and related compositions, materials, methods and systems (2019-10-01). CALIFORNIA INSTITUTE OF TECHNOLOGY [US]. Inventors: Julia A. Kornfield [US], Mark E. Davis [US], Ming-Hsin Wei [US], Simon C. Jones [US].

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Polymer Molecular Weight Analysis

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Weight-average (M_w) and number-average molecular weight (M_n) values and molecular weight distributions (M_w/M_n) values of the polymers were evaluated using a Jasco LC-2000Plus gel permeation chromatograph (GPC) equipped with a refractive index detector RI-2031Plus (Jasco, Oklahoma City, OK, USA) using 3 Agilent (Santa Clara, CA, USA) PLgel columns, 5 × 10⁻⁶ m particle size, 300 × 7.5 mm (M_w range: 5 × 10² to 17 × 10⁵ g·mol⁻¹). THF was chosen as eluent at a flow rate of 0.5 mL·min⁻¹ at 35 °C. The GPC samples were injected using a Jasco AS-2055Plus autosampler. The instrument was calibrated using polystyrene standards from 580 to 3,250,000 Da (Polymer Laboratories, Church Stretton, UK). Probes have been run in duplicates, showing full consistency and overlapping of the data.

Cingolani A., Casalini T., Caimi S., Klaue A., Sponchioni M., Rossi F, & Perale G. (2018). A Methodologic Approach for the Selection of Bio-Resorbable Polymers in the Development of Medical Devices: The Case of Poly(l-lactide-co-ε-caprolactone). Polymers, 10(8), 851.

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Determination of PLA Molecular Weight by GPC

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To measure the PLA samples number-average molecular weight (

\bar{M_{n}}

) and weight average molecular weight (

\bar{M_{w}}

), we used gel permeation chromatography (Agilent PL-GPC 50 System, Santa Clara, CA, USA). The samples were dissolved in chloroform and filtered through a PTFE filter. Four Agilent PL-Gel columns at 30 °C (3 x PL-Gel Mixed C (5 μm) and 1 x PL-Gel Mixed E (3 μm) columns) were used in series, with amylene-stabilized HPLC grade chloroform as the eluent (flow rate of 1 mL/(1/min)), on a Waters Alliance system equipped with an Alliance 2695 Separation Module. Polymer number-average molecular weight (

\bar{M_{n}}

) and polydispersity index (

\bar{M_{w}}

\bar{M_{n}}

; PDI) were calibrated against low dispersity polystyrene standards with a 3rd order polynomial fit, linear across molar mass ranges.

Kmetty Á, & Litauszki K. (2020). Development of Poly (Lactide Acid) Foams with Thermally Expandable Microspheres. Polymers, 12(2), 463.

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Synthesis and Characterization of Polycaprolactone

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All manipulations were performed
in an MBRAUN stainless steel glovebox equipped with a gas purification
system under a nitrogen atmosphere. All chemicals were purchased from
Fisher Scientific and used as received unless stated otherwise. Toluene
and THF were dried on an Innovated Technologies solvent purification
system with alumina columns and nitrogen working gas. Benzene-d₆ was supplied by Cambridge Isotope Laboratories
and distilled from CaH₂ under a nitrogen atmosphere. δ-Valerolactone
(VL; 99%) and ε-caprolactone (CL; 99%) were distilled from CaH₂ under high vacuum. Benzyl alcohol was distilled from CaH₂ under high vacuum. l-Lactide was supplied by Acros
Organics and recrystallized from dry toluene prior to use. 1-[3,5-Bis(trifluoromethyl)phenyl]-3-cyclohexylthiourea
(1) was synthesized and purified according to literature
procedures.⁴ 1,8-Diazabicyclo[5.4.0]undec-7-ene
(DBU) and 7-methyl-1,5,7-triazabicyclo[4.4.0]dec-5-ene (MTBD) were
purchased from TCI. NMR experiments were performed on a Bruker Avance
300 MHz spectrometer. Size exclusion chromatography (SEC) was performed
at 40 °C in dichloromethane (DCM) using an Agilent Infinity GPC
system equipped with three Agilent PLGel columns 7.5 mm × 300
mm (5 μm, pore sizes: 10³, 10⁴, and 10⁵ Å). Molecular weight and M_w/M_n were determined versus PS standards
(500 g/mol–3150 kg/mol; Polymer Laboratories).

Kazakov O.I., Datta P.P., Isajani M., Kiesewetter E.T, & Kiesewetter M.K. (2014). Cooperative Hydrogen-Bond Pairing in Organocatalytic Ring-Opening Polymerization. Macromolecules, 47(21), 7463-7468.

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Molecular Weight Characterization of Polymers

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Example 9

MALLS, i.e. Multi-angle Laser Light Scattering, was used in conjunction with GPC to determine the molecular weights and polydispersity of the polymers. The system used a Wyatt DAWN EOS multi-angle laser light scattering detector (λ=690 nm) with a Waters 410 differential refractometer (RI) (λ=930 nm) connected in series. Chromatographic separation by the size exclusion principle (largest comes out first) was achieved by using four Agilent PLgel columns (pore sizes 10³, 10⁴, 10⁵, and 10⁶Å) connected in series. Degassed THF was used as the mobile phase with a temperature of 35° C. and a flow rate of 0.9 ml/min. The time for complete elution through the system was 50 min, and MALLS and RI data were recorded at 5 Hz.

Samples were prepared by dissolving 5 mg of polymer in 1 ml of THF and filtering the solution through 0.45 m PTFE membrane syringe filters immediately before injection. An injection volume of 20 μl was used. The data were analyzed by Wyatt Astra Software (version 5.3.4) using the Zimm fitting formula with dn/dc=0.125 for PCOD in THF to obtain weight-average molecular weight (M_w) for each polymer reported.

US10781150B2. Molecular sieves mediated unsaturated hydrcarbon separation and related compositions, materials, methods and systems (2020-09-22). CALIFORNIA INSTITUTE OF TECHNOLOGY [US]. Inventors: Julia A. Kornfield [US], Mark E. Davis [US], Ming-Hsin Wei [US], Simon C. Jones [US].

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Gel Permeation Chromatography with MALS

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GPC with THF as mobile phase was conducted using a Shimadzu system fitted with a Wyatt DAWN DSP multi-angle laser light scattering detector (690 nm, 30 mW) and a Wyatt OPTILAB EOS interferometric refractometer (690 nm). Three Agilent PLgel columns (MIXED-C; 5 μm bead size) were employed, operating at 1 mL per minute at a column temperature of 45 °C. To process the GPC data, the program ‘Astra’ by Wyatt technologies was used. All samples were filtered through 0.45 μm nylon filters prior to injection. When aqueous-phase GPC was employed, a separate Shimadzu liquid chromatography system was utilized, equipped with a Shimadzu RID-10 refractometer (λ = 633 nm), using three Waters Ultrahydrogel columns in series ((i) 250 Å porosity, 6 μm diameter bead size; (ii) and (iii) linear, 10 μm diameter bead size), operating at room temperature. The eluent was Milli-Q water containing 20% v/v acetonitrile and 0.1% w/v TFA at a flow rate of 0.5 mL·min⁻¹. The molecular weight of the analyte was determined using a calibration based on narrow molecular weight distribution poly(ethylene glycol) standards.

Fu Q., McKenzie T.G., Ren J.M., Tan S., Nam E, & Qiao G.G. (2016). A novel solid state photocatalyst for living radical polymerization under UV irradiation. Scientific Reports, 6, 20779.

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Preparation and Characterization of Polylactide

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All manipulations were performed in an MBRAUN stainless steel glovebox equipped with a gas purification system under a nitrogen atmosphere. All chemicals were purchased from Fisher Scientific and used as received unless stated otherwise. Dichloromethane, toluene and THF (HPLC grade) were dried on an Innovative Technology solvent purification system with activated alumina columns. Thiourea catalysts were prepared as previously described.^{7 ,15} L-lactide and RAC-lactide from Acros Organics were recrystallized from dry toluene prior to use. Benzyl alcohol was distilled from CaH₂ under high vacuum. Dialysis bags (MWCO = 3,000) were purchased from SpectraPor and stored in aqueous NaN₃ solution. NMR experiments were performed on a Bruker Avance 300 MHz spectrometer except decoupled experiments which were performed on a Varian 500 MHz NMR spectrometer. Size exclusion chromatography (SEC) was performed at 30 °C in dichloromethane (DCM) at 1.0 mL/min using a Agilent Infinity GPC system equipped with three Agilent PLGel columns 7.5 mm ×300 mm (5 μm; pore sizes = 10³, 10⁴, and 10⁵ Å) and multiwavelength detector (set to 254 nm) and refractive index detector connected in series. Molecular weight and M_w/M_n were determined versus PS standards (500 g/mol to 3150 kg/mol; Polymer Laboratories). MALDI–TOF data was acquired at the University of Akron Mass Spectrometry Center.

Spink S.S., Kazakov O.I., Kiesewetter E.T, & Kiesewetter M.K. (2015). Rate Accelerated Organocatalytic Ring-Opening Polymerization of L-Lactide via the Application of a Bis(thiourea) H-bond Donating Cocatalyst. Macromolecules, 48(17), 6127-6131.

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Molecular Weight Characterization of Polymers

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Example 9

MALLS, i.e. Multi-angle Laser Light Scattering, was used in conjunction with GPC to determine the molecular weights and polydispersity of the polymers. The system used a Wyatt DAWN EOS multi-angle laser light scattering detector (λ=690 nm) with a Waters 410 differential refractometer (RI) (λ=930 nm) connected in series. Chromatographic separation by the size exclusion principle (largest comes out first) was achieved by using four Agilent PLgel columns (pore sizes 10³, 10⁴, 10⁵, and 10⁶Å) connected in series. Degassed THF was used as the mobile phase with a temperature of 35° C. and a flow rate of 0.9 ml/min. The time for complete elution through the system was 50 min, and MALLS and RI data were recorded at 5 Hz.

US10112878B2. Molecular sieves mediated unsaturated hydrocarbon separation and related compositions, materials, methods and systems (2018-10-30). CALIFORNIA INSTITUTE OF TECHNOLOGY [US]. Inventors: Julia A. Kornfield [US], Mark E. Davis [US], Ming-Hsin Wei [US], Simon C. Jones [US].

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Characterization of Triblock Copolymer Structure

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The triblock was mixed with KBr, and then its structure was also confirmed by the Fourier transform infrared analysis (FTIR) (vertex 70, Bruker, Germany) [23, 30] .
Polydispersity Index To determine the polydispersity index (PDI), average molecular weight (M w ), and the number average molecular weight (M n ) of the synthesized triblock, a GPC-Addon apparatus with Plgel® columns (Agilent, USA) was used. In the GPC technique, tetrahydrofuran as eluent at a flow rate of 1 mL/min was employed, and polystyrene was used as a standard [23] .
Differential Scanning Calorimetry To identify the glass transition and melting temperatures of triblock, differential scanning calorimetry (DSC) was conducted by a DSC822 (Mettler Toledo, Switzerland). Approximately, a few mg of samples (3-4 mg) were accurately weighed into aluminum pans and then sealed. The pans were cooled down to -60 °C followed by heating the samples to 60 °C at a scanning rate of 5 °C/min under nitrogen atmosphere.

Kamali H., Khodaverdi E., Kaffash E., Saffari A.S., Shiadeh S.N.R., Nokhodchi A., & Hadizadeh F. (2020). Optimization and in Vitro Evaluation of Injectable Sustained-Release of Levothyroxine Using PLGA-PEG-PLGA. Journal of Pharmaceutical Innovation, 16(4), 688-698.

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